1H-1,2,4-Triazole → HCID 10946371、化合物

HRID 1742117ノート

反応式

HRID 1742117 の反応式
[NH:1]1[CH:5]=[N:4][CH:3]=[N:2]1.Cl[CH2:7][C:8]([C:18]1([F:21])[CH2:20][CH2:19]1)([OH:17])[CH2:9][C:10]1[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][CH:11]=1>CN(C)C=O>[Cl:16][C:13]1[CH:12]=[CH:11][C:10]([CH2:9][C:8]([C:18]2([F:21])[CH2:19][CH2:20]2)([OH:17])[CH2:7][N:1]2[CH:5]=[N:4][CH:3]=[N:2]2)=[CH:15][CH:14]=1

参加物

4

反応物 2

HCID 92571H-1,2,4-TriazoleHCID 110973804-Chloro-α-(chloromethyl)-α-(1-fluorocyclopropyl)benzeneethanol

生成物 1

HCID 10946371HCID 10946371、化合物収率 35%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
80 °C

実験手順

Under an atmosphere of nitrogen, 27.6 g (0.4 mol) of 1,2,4-triazole and 33.6 g (0.3 mol) of potassium tert.-butylate in 100 ml of absolute dimethylformamide are introduced as an initial charge and heated to 80° C. At this temperature, a solution of 26.3 g (0.1 mol) of 1-chloro-2-(1-fluoro-cyclopropyl)-3-(4-chlorophenyl)-propan-2-ol in 50 ml of absolute dimethylformamide is added dropwise thereto while stirring. The mixture is stirred for another 6 hours at 100° C. and then concentrated by stripping off the diluent under reduced pressure. The residue is taken up in ethyl acetate, the solution is washed with water, and, after drying over sodium sulphate, the solvent is evaporated under reduced pressure. The product left behind is chromatographed on a silica gel column, using chloroform as the mobile solvent. In this way, 8.9 g (35% of theory) of 1-(4-chlorophenyl)-2-(1-fluoro-cyclopropyl)-3-(1,2,4-triazol-1-yl)-propan-2-ol are obtained in the form of a solid.

後処理

  1. additionan initial charge
  2. stirringThe mixture is stirred for another 6 hours at 100° C.
  3. concentrationconcentrated
  4. washthe solution is washed with water
  5. dry with materialafter drying over sodium sulphate
  6. customthe solvent is evaporated under reduced pressure
  7. waitThe product left behind
  8. customis chromatographed on a silica gel column

出典と根拠

ORDレコード
ord-4ba2c8fc4e584fbaa41b104b8df6b260
出典データセット
uspto-grants-1994_08
特許番号
US05336809

反応ノート

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